HRID392227

反应详情

EQUATION

反应方程式

HRID 392227 的结构方程式

AUXILIARIES

试剂、催化剂与溶剂

3

CONDITIONS

反应条件

温度
110 °C

PROCEDURE

实验过程

A solution of methyl 3-iodo-4-(3-methyl-but-2-enylamino)-benzoate (2.0 g, Reference Example 53) in triethylamine (1.6 ml) and acetonitrile (35 ml) was treated with palladium acetate (0.05 g). The mixture was sealed in a bomb and heated at 110° C. for 18 hours. After cooling the reaction mixture was filtered and the filtrate was evaporated. The residue was subjected to flash chromatography on silica eluting with a mixture of ethyl acetate and petroleum ether (1:4, v/v) to give the title compound (1.0 g).

WORKUP

后处理

  1. customThe mixture was sealed in a bomb
  2. temperatureAfter cooling the reaction mixture
  3. filtrationwas filtered
  4. customthe filtrate was evaporated
  5. additionThe residue was subjected to flash chromatography on silica eluting with a mixture of ethyl acetate and petroleum ether (1:4, v/v)